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MoS2 solids were prepared through the formulation and thermal decomposition of water in oil emulsions (W/O), using ammonium heptamolybdate ((NH4)6Mo7O24.4H2O) and a sulfur agent, for the assessment of potential active phases feasible in novel ultradispersed catalysts for the conversion of hydrocarbons. The solids were characterized by (XPS), temperature programmed oxidation (TPO), and elemental analysis. XPS results revealed materials with surfaces enriched in sulphur, as well as a considerable stability to the oxidation by ambient exposure. Results evidenced that the amount of sulphur included in the emulsion aqueous phase is crucial to control the stoichiometry of the solids synthesized by this methodology. TPO profiles showed different types of S and C suggesting that this elements trend to react simultaneously, indicating that carbon is intimately associated to the sulphur in the structure of the solids.